US7608118B2 - Preconditioning fuel cell membrane electrode assemblies - Google Patents

Preconditioning fuel cell membrane electrode assemblies Download PDF

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Publication number
US7608118B2
US7608118B2 US10/988,811 US98881104A US7608118B2 US 7608118 B2 US7608118 B2 US 7608118B2 US 98881104 A US98881104 A US 98881104A US 7608118 B2 US7608118 B2 US 7608118B2
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Prior art keywords
fuel cell
membrane electrode
cell membrane
electrode assembly
typically
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Expired - Fee Related, expires
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US10/988,811
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US20060105214A1 (en
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Bradley P. Anderson
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3M Innovative Properties Co
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3M Innovative Properties Co
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Assigned to 3M INNOVATIVE PROPERTIES COMPANY reassignment 3M INNOVATIVE PROPERTIES COMPANY ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: ANDERSON, BRADLEY P.
Priority to US10/988,811 priority Critical patent/US7608118B2/en
Priority to KR1020077010863A priority patent/KR20070085347A/ko
Priority to PCT/US2005/036640 priority patent/WO2006055124A1/en
Priority to EP05808870A priority patent/EP1825548A1/en
Priority to JP2007541187A priority patent/JP2008521168A/ja
Priority to CN2005800390887A priority patent/CN101057360B/zh
Priority to TW094137371A priority patent/TW200623491A/zh
Publication of US20060105214A1 publication Critical patent/US20060105214A1/en
Publication of US7608118B2 publication Critical patent/US7608118B2/en
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M8/00—Fuel cells; Manufacture thereof
    • H01M8/10—Fuel cells with solid electrolytes
    • H01M8/1004—Fuel cells with solid electrolytes characterised by membrane-electrode assemblies [MEA]
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
    • H01M4/88—Processes of manufacture
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M8/00—Fuel cells; Manufacture thereof
    • H01M8/04—Auxiliary arrangements, e.g. for control of pressure or for circulation of fluids
    • H01M8/04298—Processes for controlling fuel cells or fuel cell systems
    • H01M8/043—Processes for controlling fuel cells or fuel cell systems applied during specific periods
    • H01M8/04302—Processes for controlling fuel cells or fuel cell systems applied during specific periods applied during start-up
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M8/00—Fuel cells; Manufacture thereof
    • H01M8/04—Auxiliary arrangements, e.g. for control of pressure or for circulation of fluids
    • H01M8/04082—Arrangements for control of reactant parameters, e.g. pressure or concentration
    • H01M8/04089—Arrangements for control of reactant parameters, e.g. pressure or concentration of gaseous reactants
    • H01M8/04119—Arrangements for control of reactant parameters, e.g. pressure or concentration of gaseous reactants with simultaneous supply or evacuation of electrolyte; Humidifying or dehumidifying
    • H01M8/04126—Humidifying
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/30—Hydrogen technology
    • Y02E60/50—Fuel cells
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T29/00—Metal working
    • Y10T29/49—Method of mechanical manufacture
    • Y10T29/49002—Electrical device making
    • Y10T29/49108—Electric battery cell making
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T29/00—Metal working
    • Y10T29/49—Method of mechanical manufacture
    • Y10T29/49002—Electrical device making
    • Y10T29/49108—Electric battery cell making
    • Y10T29/4911—Electric battery cell making including sealing

Definitions

  • This invention relates to a method of preconditioning fuel cell membrane electrode assemblies for use in fuel cell systems which includes exposure to saturated steam at superatmospheric pressures.
  • the present invention provides a method of preconditioning a fuel cell membrane electrode assembly comprising the steps of: a) providing a fuel cell membrane electrode assembly; and b) exposing the fuel cell membrane electrode assembly to saturated steam at a treatment pressure which is at least 110 kPa, more typically at least 130 kPa, more typically at least 170 kPa, and most typically at least 200 kPa.
  • the duration of step b) is typically at least 10 minutes and more typically at least 25 minutes.
  • the method may or may not include the additional step of enclosing the fuel cell membrane electrode assembly in a container, which may or may not be impervious to water or substantially impervious to water, within 96 hours after step b), more typically within 1 hour after step b), more typically after step b) but before the fuel cell membrane electrode assembly returns to ambient temperature.
  • the container may or may not include a humidifying element.
  • FIG. 1 is a graph containing log plots of potentiodynamic scans at various voltages for an MEA preconditioned according to the present invention.
  • FIG. 2 is a graph containing log plots of potentiodynamic scans at various voltages for a comparative non-preconditioned MEA.
  • FIG. 3 is a graph containing log plots of potentiodynamic scans at various voltages for a comparative non-preconditioned MEA.
  • the present invention provides a method for preconditioning fuel cell membrane electrode assemblies (MEA's).
  • the preconditioning method according to the present invention results in reduction of the start up or conditioning time required when the MEA's are first installed in a fuel cell system and improvement of overall performance, as reflected in the achievement of high current density at relatively high voltage.
  • a membrane electrode assembly is the central element of a proton exchange membrane fuel cell, such as a hydrogen fuel cell.
  • Fuel cells are electrochemical cells which produce usable electricity by the catalyzed combination of a fuel such as hydrogen and an oxidant such as oxygen.
  • Typical MEA's comprise a polymer electrolyte membrane (PEM) (also known as an ion conductive membrane (ICM)), which functions as a solid electrolyte.
  • PEM polymer electrolyte membrane
  • ICM ion conductive membrane
  • Each electrode layer includes electrochemical catalysts, typically including platinum metal.
  • GDL Gas diffusion layers
  • FTL fluid transport layer
  • DCC diffuser/current collector
  • the anode and cathode electrode layers may be applied to GDL's in the form of a catalyst ink, and the resulting coated GDL's sandwiched with a PEM to form a five-layer MEA.
  • the anode and cathode electrode layers may be applied to opposite sides of the PEM in the form of a catalyst ink, and the resulting 3-layer MEA sandwiched with two GDL's to form a five-layer MEA.
  • the 3-layer MEA may also be called a catalyst-coated membrane (CCM).
  • the five layers of a five-layer MEA are, in order: anode GDL, anode electrode layer, PEM, cathode electrode layer, and cathode GDL.
  • a 7-layer MEA may be made by addition of appropriate gaskets to each side of a 5-layer MEA.
  • MEA's may additionally include other functional layers, which might include hard stops, hydrophilic or hydrophobic coatings, adhesives, and the like.
  • MEA Any suitable MEA may be used in the practice of the present invention, including 3-, 5- and 7-layer MEA's with or without GDL's, gaskets, hard stops, hydrophilic or hydrophobic coatings, adhesives, and the like.
  • the MEA may comprise any suitable PEM, including non-fluorinated, highly fluorinated and perfluorinated PEM's with or without support matrices, such as porous PTFE support matrices.
  • the PEM may comprise any suitable polymer electrolyte.
  • Typical polymer electrolytes useful in fuel cells bear anionic functional groups bound to a common backbone, which are typically sulfonic acid groups but may also include carboxylic acid groups, imide groups, amide groups, or other acidic functional groups.
  • Typical polymer electrolytes are copolymers of tetrafluoroethylene and one or more fluorinated, acid-functional comonomers.
  • Typical polymer electrolytes include NAFION® (DuPont Chemicals, Wilmington Del.) and FLEMIONTM (Asahi Glass Co. Ltd., Tokyo, Japan).
  • the polymer electrolyte may be a copolymer of tetrafluoroethylene (TFE) and FSO 2 —CF 2 CF 2 CF 2 CF 2 —O—CF ⁇ CF 2 , described in U.S. patent application Ser. Nos. 10/322,254, 10/322,226 and 10/325,278, which are incorporated herein by reference.
  • the polymer typically has an equivalent weight (EW) of 1200 or less, more typically 1100 or less, more typically 1000 or less, and more typically 900 or less.
  • EW equivalent weight
  • membranes useful in the present invention include hydrocarbon polymers, including aromatic polymers.
  • useful hydrocarbon polymers include sulfonated polyetheretherketone, sulfonated polysulfone, and sulfonated polystyrene.
  • the polymer can be formed into a PEM by any suitable method.
  • the polymer is typically cast from a suspension. Any suitable casting method may be used, including bar coating, spray coating, slit coating, brush coating, and the like.
  • the membrane may be formed from neat polymer in a melt process such as extrusion. After forming, the membrane may be annealed, typically at a temperature of 120° C. or higher, more typically 130° C. or higher, most typically 150° C. or higher.
  • the PEM typically has a thickness of less than 50 microns, more typically less than 40 microns, more typically less than 30 microns, and most typically about 25 microns.
  • any suitable catalyst may be used in the practice of the present invention.
  • carbon-supported catalyst particles are used. Typical carbon-supported catalyst particles are 50-90% carbon and 10-50% catalyst metal by weight, the catalyst metal typically comprising Pt for the cathode and Pt and Ru in a weight ratio of 2:1 for the anode.
  • the catalyst is applied to the PEM or to the FTL in the form of a catalyst ink. Alternately, the catalyst ink may be applied to a transfer substrate, dried, and thereafter applied to the PEM or to the FTL as a decal.
  • the catalyst ink typically comprises polymer electrolyte material, which may or may not be the same polymer electrolyte material which comprises the PEM.
  • the catalyst ink typically comprises a dispersion of catalyst particles in a dispersion of the polymer electrolyte.
  • the ink typically contains 5-30% solids (i.e. polymer and catalyst) and more typically 10-20% solids.
  • the electrolyte dispersion may be in any suitable solvent system.
  • the electrolyte dispersion is typically an aqueous dispersion, which may additionally contain NMP (n-methyl-2-pyrrolidone), alcohols or polyalcohols such a glycerin and ethylene glycol.
  • the water, alcohol, and polyalcohol content may be adjusted to alter rheological properties of the ink.
  • the ink typically contains 0-50% alcohol and 0-20% polyalcohol.
  • the ink may contain 0-2% of a suitable dispersant.
  • the ink is typically made by stirring with heat followed by dilution to a coatable consistency.
  • the MEA may comprise nanostructured catalysts on high-aspect ratio supports as described in U.S. Pat. Nos. 6,425,993, 6,042,959, 6,042,959, 6,319,293, 5,879,828, 6,040,077 and 5,879,827 and U.S. patent application Ser. No. 10/674,594, incorporated herein by reference.
  • catalyst may be applied to the PEM by any suitable means, including both hand and machine methods, including hand brushing, notch bar coating, fluid bearing die coating, wire-wound rod coating, fluid bearing coating, slot-fed knife coating, three-roll coating, or decal transfer. Coating may be achieved in one application or in multiple applications.
  • catalyst may be applied to the GDL by any suitable means, including both hand and machine methods, including hand brushing, notch bar coating, fluid bearing die coating, wire-wound rod coating, fluid bearing coating, slot-fed knife coating, three-roll coating, or decal transfer. Coating may be achieved in one application or in multiple applications.
  • any suitable GDL may be used in the practice of the present invention.
  • the GDL is comprised of sheet material comprising carbon fibers.
  • the GDL is a carbon fiber construction selected from woven and non-woven carbon fiber constructions.
  • Carbon fiber constructions which may be useful in the practice of the present invention may include: TORAYTM Carbon Paper, SPECTRACARBTM Carbon Paper, AFNTM non-woven carbon cloth, ZOLTEKTM Carbon Cloth, and the like.
  • the GDL may be coated or impregnated with various materials, which may include carbon particle coatings, hydrophilizing treatments, and hydrophobizing treatments such as coating with polytetrafluoroethylene (PTFE).
  • PTFE polytetrafluoroethylene
  • GDL's may be applied to either side of a CCM by any suitable means.
  • catalyst coated GDL's may be applied to either side of a PEM by any suitable means.
  • an MEA is exposed to saturated steam at superatmospheric pressures.
  • Saturated steam is steam at the temperature of its boiling point, for its given pressure.
  • Saturated steam can co-exist with water at the same temperature and pressure.
  • the temperature and pressure of saturated steam have a fixed relationship; given one value, the other can be calculated.
  • the pressure is at least 110 kPa (corresponding to a temperature of at least 102.3° C.), more typically at least 130 kPa (corresponding to a temperature of at least 107.1° C.), more typically at least 150 kPa (corresponding to a temperature of at least 111.4° C.), more typically at least 170 kPa (corresponding to a temperature of at least 115.2° C.), more typically at least 190 kPa (corresponding to a temperature of at least 118.7° C.), and most typically at least 200 kPa (corresponding to a temperature of at least 120.2° C.).
  • treatment conditions are chosen so as to avoid any heat damage to the MEA that results in undesirable overall performance of the MEA.
  • treatment apparatus including autoclaves, pressure cookers, and the like. Any suitable water or steam sources may be used. Treatment apparatus adapted for continuous or batch-wise treatment may be used.
  • duration of treatment is at least one minute, more typically at least 5 minutes, more typically at least 10 minutes, more typically at least 15 minutes, and more typically at least 25 minutes.
  • duration of treatment may be reduced when thinner MEA's or higher pressures are used.
  • the preconditioned MEA is sealed or enclosed in a container shortly after treatment.
  • this container contains a humidifying element as disclosed in copending U.S. patent application Ser. No. 10/988,740, filed on Nov. 15, 2004, published as U.S. patent publication 2004/0105219-A1 on May 18, 2006, the disclosure of which is incorporated herein by reference.
  • the container may be made of any suitable material, which may be impervious to water, substantially impervious to water, airtight, substantially airtight, modified atmosphere packaging, watertight, substantially watertight or none of the above. “Impervious to water” means impervious to both liquid water and water vapor.
  • the material of the container is impervious to water or substantially impervious to water.
  • the material of the container may be rigid or flexible.
  • the material of the container may be single- or multiwall.
  • the interior of the container may optionally comprise release materials or coatings.
  • the preconditioned MEA is enclosed in the container after treatment and before returning to ambient temperature.
  • the preconditioned MEA is enclosed in the container within 10 minutes of treatment.
  • the preconditioned MEA is enclosed in the container within 1 hour of treatment.
  • the preconditioned MEA is enclosed in the container within 24 hours of treatment.
  • the preconditioned MEA is enclosed in the container within 96 hours of treatment.
  • the preconditioned MEA is used to assemble a fuel cell stack shortly after treatment.
  • this stack includes a humidifying element as disclosed in copending U.S. patent application Ser. No. 10/988,740, filed on Nov. 15, 2004, published as U.S. patent publication 2004/0105219-A1 on May 18, 2006, the disclosure of which is incorporated herein by reference.
  • the preconditioned MEA is incorporated into a fuel cell stack after treatment and before returning to ambient temperature (typically room temperature).
  • the preconditioned MEA is incorporated into a fuel cell stack within 10 minutes of treatment.
  • the preconditioned MEA is incorporated into a fuel cell stack within 1 hour of treatment.
  • the preconditioned MEA is incorporated into a fuel cell stack within 24 hours of treatment.
  • the preconditioned MEA is incorporated into a fuel cell stack within 96 hours of treatment.
  • This invention is useful in the manufacture and operation of fuel cells.
  • 5-layer MEA's having 50 cm 2 of active area were prepared as follows. Catalyst dispersions were prepared according to the method described in WO 2002/061,871, incorporated herein by reference. To prepare catalyst-coated membranes, anode and cathode layers were applied to membranes according to the decal transfer method described in the same reference, WO 2002/061,871. PTFE-treated carbon paper gas diffusion layers and polytetrafluoroethylene/glass composite gaskets were applied to the CCM by pressing in a Carver Press (Fred Carver Co., Wabash, IN.) with 13.4 kN of force at 132° C. for 10 minutes.
  • Carver Press Frred Carver Co., Wabash, IN.
  • the preconditioned MEA was mounted in a test station with independent controls of gas flow, pressure, relative humidity, and current or voltage (Fuel Cell Technologies, Albuquerque, N. Mex.).
  • the test fixture included graphite current collector plates with quad-serpentine flow fields.
  • the anode gas was 800 sccm H 2 and the cathode gas was 1800 sccm air, with 100% RH in both anode and cathode gases.
  • Cell temperature was 70° C.
  • the test protocol holds the cell at 0.5 V for 10 minutes and then runs a potentiodynamic scan (PDS) from 0.9 Volts to 0.3 volts, holding for about 5 seconds per point and using 0.05 volt increments.
  • PDS potentiodynamic scan
  • FIGS. 2 and 3 are a similar plots taken in the same manner for comparative MEA's which were identical except that they were not preconditioned.
  • FIG. 1 A comparison of FIG. 1 with FIGS. 2 and 3 indicates that the preconditioned MEA started up faster than the non-conditioned MEA's. Note that flooding of the MEA may dominate the voltage performance at higher current densities, and therefore the data collected at middle- or low range current densities may better reflect the voltage performance of the MEA.
  • the 0.8V and 0.7V traces of FIGS. 1-3 demonstrate not only superior start up performance for the preconditioned MEA but also superior performance as reflected in higher current density achieved at a given voltage.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Sustainable Development (AREA)
  • Sustainable Energy (AREA)
  • Fuel Cell (AREA)
  • Inert Electrodes (AREA)
US10/988,811 2004-11-15 2004-11-15 Preconditioning fuel cell membrane electrode assemblies Expired - Fee Related US7608118B2 (en)

Priority Applications (7)

Application Number Priority Date Filing Date Title
US10/988,811 US7608118B2 (en) 2004-11-15 2004-11-15 Preconditioning fuel cell membrane electrode assemblies
JP2007541187A JP2008521168A (ja) 2004-11-15 2005-10-11 燃料電池膜電極接合体の前調整
PCT/US2005/036640 WO2006055124A1 (en) 2004-11-15 2005-10-11 Preconditioning fuel cell membrane electrode assemblies
EP05808870A EP1825548A1 (en) 2004-11-15 2005-10-11 Preconditioning fuel cell membrane electrode assemblies
KR1020077010863A KR20070085347A (ko) 2004-11-15 2005-10-11 연료 전지 멤브레인 전극 조립체를 사전조정하는 방법
CN2005800390887A CN101057360B (zh) 2004-11-15 2005-10-11 预处理的燃料电池膜电极组件
TW094137371A TW200623491A (en) 2004-11-15 2005-10-25 Preconditioning fuel cell membrane electrode assemblies

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Application Number Priority Date Filing Date Title
US10/988,811 US7608118B2 (en) 2004-11-15 2004-11-15 Preconditioning fuel cell membrane electrode assemblies

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US20060105214A1 US20060105214A1 (en) 2006-05-18
US7608118B2 true US7608118B2 (en) 2009-10-27

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US (1) US7608118B2 (ko)
EP (1) EP1825548A1 (ko)
JP (1) JP2008521168A (ko)
KR (1) KR20070085347A (ko)
CN (1) CN101057360B (ko)
TW (1) TW200623491A (ko)
WO (1) WO2006055124A1 (ko)

Cited By (1)

* Cited by examiner, † Cited by third party
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US20110236774A1 (en) * 2010-03-29 2011-09-29 Korea Institute Of Energy Research System for Pre-Activation of Polymer Electrolyte Fuel Cell (PEFC)

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JP4688157B2 (ja) * 2005-12-28 2011-05-25 トヨタ自動車株式会社 燃料電池電極用触媒の製造方法
KR100811985B1 (ko) * 2007-02-15 2008-03-10 삼성에스디아이 주식회사 멀티 ｍｅａ 테스트 스테이션 및 이를 이용한 멀티 ｍｅａ평가 방법
US9053323B2 (en) 2007-04-13 2015-06-09 Hewlett-Packard Development Company, L.P. Trusted component update system and method
US8007958B2 (en) 2007-08-21 2011-08-30 GM Global Technology Operations LLC PEM fuel cell with improved water management
US20090068528A1 (en) * 2007-09-12 2009-03-12 Teasley Mark F Heat treatment of perfluorinated ionomeric membranes
WO2009068563A1 (de) * 2007-11-28 2009-06-04 Basf Se Dampfhydratisierung /speek-membran
KR102586433B1 (ko) 2018-04-26 2023-10-06 현대자동차주식회사 연료전지용 전해질막의 제조방법 및 이로 제조된 전해질막

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JP2008521168A (ja) 2008-06-19
EP1825548A1 (en) 2007-08-29
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WO2006055124A1 (en) 2006-05-26
CN101057360A (zh) 2007-10-17
KR20070085347A (ko) 2007-08-27
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